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We report on the electrical and structural properties of boron-doped diamond tips commonly used for in-situ electromechanical testing during nanoindentation. The boron dopant environment, as evidenced by cathodoluminescence (CL) microscopy, revealed significantly different boron states within each tip. Characteristic emission bands of both electrically activated and nonelectrically activated boron centers were identified in all boron-doped tips. Surface CL mapping also revealed vastly different surface properties, confirming a high amount of nonelectrically activated boron clusters at the tip surface. Raman microspectroscopy analysis showed that structural characteristics at the atomic scale for boron-doped tips also differ significantly when compared to an undoped diamond tip. Furthermore, the active boron concentration, as inferred via the Raman analysis, varied greatly from tip-to-tip. It was found that tips (or tip areas) with low overall boron concentration have a higher number of electrically inactive boron, and thus non-Ohmic contacts were made when these tips contacted metallic substrates. Conversely, tips that have higher boron concentrations and a higher number of electrically active boron centers display Ohmic-like contacts. Our results demonstrate the necessity to understand and fully characterize the boron environments, boron concentrations, and atomic structure of the tips prior to performing in situ electromechanical experiments, particularly if quantitative electrical data are required.

Monitoring with an Acoustic Emission (AE) sensor integrated into an indenter tip was utilized for the evaluation of the earliest stages of indentation-induced plasticity in sapphire single crystal. The evaluated surfaces included basal (C), rhombohedral (R) and two different prismatic orientations (A and M). The differences between the mechanisms of the initial stages of plasticity for the various crystallographic orientations were reflected in the following aspects of AE activity: detection of a specific type of AE waveform that correlated to the presence of linear surface features near the indentation impressions; AE signal associated with the yield point, consisting either of one or two distinct waveforms; and presence or absence of AE signals after the yield point. Moreover, analysis of AE activity revealed loading rate effects on the yield point mechanism for the M plane. The possibility of plasticity onset mechanisms involving both slip and twinning is discussed.

For many years, a fundamental problem in contact mechanics, both tribology and indentation problems, has been the inability to see what is taking place—the buried-interface problem. Over the past few years, there have been developments whereby it has become possible to perform contact mechanics experiments in situ within a transmission electron microscope. These new experiments have been enabled by both the miniaturization of sensors and actuators and improvements in their mechanical stability and force sensitivity. New information is now becoming available about the nanoscale processes of sliding, wear, and tribochemical reactions, as well as microstructural evolution during nanoindentation such as dislocation bursts and phase transformations. This article provides an overview of some of these developments, in terms of both the advances in technical instrumentation and some of the novel scientific insights.

Testing the mechanical properties of nanoscale materials faces a number of inherent challenges. As the size of the “target” decreases, the inability to actually see what occurs during testing can be troublesome. While a number of studies have attempted to characterize the mechanical response of nanoscale materials using traditional nanoindentation techniques, certain lingering questions have always remained. For example, the nature and sequence of failure events in the case of multilayer films has long been the subject of scientific debate. Similarly, in the case of individual nanoparticles, it is often difficult to ascertain that contact was both made and maintained throughout the test. Further, the crystallographic orientation of the sample and/or the presence of preexisting defects, which can have a significant influence on mechanical properties at the nanoscale, typically remain unknown.

This study evaluated a novel approach for acoustic emission (AE) monitoring of nanoindentation. The technique utilizes a miniature AE sensor integrated into a calibrated diamond indenter tip on a commercial nanoindentation system. The evaluation focused on the yield -point phenomenon in W (100); MgO (100); and sapphire C (0001); R (1012); A (1210); and M (1010) single-crystal surfaces. The minimum amount of elastic energy release sufficient to produce AE signal detectable with the indenter tip sensor was nearly two orders of magnitude lower than the minimum energy level required for conventional AE sensors. Wave forms detected with the indenter tip sensor were independent of sample size. A linear relationship between released elastic energies and the corresponding AE energies was observed for all three evaluated materials. The scaling coefficient of the linear relationship was independent of indenter tip size/shape and indentation depth. The differences between the mechanisms of the initial stages of plasticity for the various crystallographic orientations of sapphire were reflected in the following aspects of AE activity: detection of a specific type of AE wave form that correlated to the presence of linear surface features near the indentation sites; AE signal associated with the yield point, consisting either of one or two distinct wave forms; and presence or absence of AE signals after the yield point. The possibility of plasticity onset in sapphire involving both slip and twinning is discussed.

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